Treatment of textile materials



Patented Feb. 23, 1937 PATENT OFFICE 2,011,; TREATMENT or TEXTILE MATERIALS Edward 3. Bell, Lowell, Mam, assignor to The Buromln Company, Pittsburgh, Pa., a corporation of Pennsylvania Serial No. 680,151

No Drawing. Application July 12, 1933,

2 Claims.

The present invention relates to the treatment of textiles and, more particularly, to the dyeing of textiles by the use of dilute solutions of alkalimetal hexametaphosphates.

5 In dyeing, the textile fibers employed are or animal or vegetable origin or of artificial preparation. Examples oi the first are wool and silk; oi the second, cotton and linen; of the third, rayon or other forms or artificial silk made by 10 various processes.

- Textile fibers may be dyed between any of the steps used in the manufacture of the finished fabnic, namely, they maybe dyed in the form or stock, either raw or previously scoured, in the 15 form of partially or fully combed but untwisted fiber, known as sliver or slubbing, in the form of twisted thread or yarn, or finally in the completely woven piece.

When dyed at any 01 the steps prior to weav- 2 ing, the object to be attained is the dyeing oi the material to an even shade and of the color desired. When dyed in the woven piece, this same end is striven for. On other occasions; however, where the woven piece is composed of 85 threads or different classes of fibers which have diflerent aflinities for certain dyes, it is sometimes wished to dye the whole equally and evenly, and at others to choose such dyes or dyeing methods as will color the threads of one composition a & certain color and leave the threads of the other material a difierent color or in their original white condition.

In certain other cases, specific colored designs are given to woven cloth by printing locally there- 35 on certain pigments, dyes or the component parts of dyes and then setting the pigments or develop-v ing the dyes of which a certain essential part or parts were locally applied by subjecting the whole piece of cloth to a uniform treatment.

For the successful attainment of these desired results, there must be unhindered and even penetration of the dye and its combination with the fiber to be colored.

Penetration or the evenness thereof may be hindered by fats, waxes, oils, or metallic soaps existing either naturally in the fiber or imposed thereon by some process prior to the dyeing operation.

Penetration or the evenness thereof maybe hindered by the failure of the dyestufi itself to go into true solution or to assume a suificiently divided colloidal form in the dye bath. .Small traces of extraneous metallic impurities taken up by the dye bath from the metallic walls of. the

dye kettle or'the piping thereto may, in many cases, have most serious results in dulling' or otherwise modifying the color produced by the dye. At other times, certain metallic salts are deliberately added to the dye bath or else precipitated on the material to be dyed, either prior to the dyeing thereof or subsequently thereto, for the purpose of firmly fixing the dye to the fiber or for changing the color produced otherwise by the dye alone,to a more desired one.

The following are specific cases of my new method or dyeing. A 30% solution of sodium hexametaphosphate was employed. In some cases, it was adjusted by the addition of small quantities of sodium carbonate and bicarbonate toraise its alkalinity slightly above theneutral point.

A. In attempting to dye rayon slubbing to a deep black, three hundred pounds of the slubbing were loaded into a dyeing machine. machine comprised a cylindrical vessel provided with a tight fitting cover. The slubbing was compressed between a perforated top and a peri'orated bottom in the dyeing vessel and treated with a standard dye liquor having at the beginning of the operation a. volume or five hundred gallons. The dye liquor was prepared by dissolving in water:

18 lbs. of the dye known as Direct deep black E. A. Ex. Color Index 581.

6 lbs. of the dye known as Diazo black B. H.

S. W. Color Index 401.

3 lbs. of the pure soap.

1 lbs. sodium carbonate.

The dyeing vessel had adjacent thereto a smaller vessel open at the top and the two were so interconnected by piping that the dye liquor in the smaller vessel could be forced by a mechanically driven pump, installed in the pipe line leading from the smaller vessel, into the top of the dyeing vessel, through the material to be dyed and re turned from the bottom of the dyeing vessel to the smaller auxiliary container.

The dye liquor could thus be continuously clr culated through the material to be dyed.

A small pipe line conveying steam entered the delivery pipe and enabled the circulating dye liquor to be gradually raised to the boiling point. As steam condensed in heating-the dye liquor and increased the volume thereof, care was taken to start with only so much liquor as would fill the dyeing vessel and a small part of. the'auxiliary,

reservoir, giving room in the balance thereof for the increase in volume of the dyeliquor.

The dyeing machine having been prepared as above, the dyeing was started at an approximate temperature of 100 to 110 F. and brought up to the, boiling point during a period or thirty minutes. The dye liquor was boiled for twenty minutes. Then, fiIteen pounds of sodium sulphate was added and the boiling continued .for twenty minutes more. Then, thirty pounds more sodium sulphate was added and the boiling continued for another twenty minutes. Then, sixty pounds more sodium sulphate was added and the boiling continued for another twuty minutes.

The dyeing The results of this dye ns attempt. were unsuccessiul. The layer oi rayon, perhaps some eight inches in depth, showed but small penetration of dyestufi. It shaded trom whitest the bottom. through various grays to the wished-for black at the top. The dye seemingly had penetrated scarcely an inch into the material.

Subsequent dyeing attempts were made, using variations in the amounts of sodium carbonate and soap, that were added and further attempts were also made using various preparations reouted to be of value in aiding dye penetration.

I then repeated the dyeing with the dye liquor made as detailed above. except tor the addition thereto or 1% quarts 30% solution oi sodium hexametaposphate. Theresults were peri'ectLv satisfactory. The "You at the end oi the operation was dyed a uniform deep black.

B. Pieces oi woven mixed goods containing besides the main body of wool, certain threads or white silk. were dyed inacid baths in tour ditierent ways. v

1. in acid dye bath alone. 2. Aiter first mordanting with a sodium dichromate. 3. Dyeing and then subsequently mordanting with sodium dichromate. ,4. Dyeing with simultaneous addition of soso dium .dichromate to the dye bath.

.l"our other pieces of simllar'goods were then as above, except there was added to the dye bath a dilute solution or sodium hexametaiphos-.

C. The addition of an alkali-metal hexametaphosphate improves the process known as cross dyeing, where certain fibers are to be dyed one color and others another color in the same dye bath. Beneficial results in changing the selec- 4 tive afiinities ot'fibers for certain dyes are obtained by the addition to the hexametaphosphate. D. I have found sodium hexametaphosphate to be an t in the evenness of dyeing in that process where a dye is first precipiated onthe fiber in an acid bath and then its color changed by the subsequent precipitation thereon of a chromium compound by the addition to the bath after the dye is exhausted. 01 sodium bichromate. The following dyeing was .made: 400 pounds worsted slubbing were dyed in 100 gallons of dye v bath made up as follows:

8% lbs. oi the dye known as Diamond blue '0 black R. B. N. high conc.', new. Color Index 202. 1?; lbs. of the dye known as Wool violet 4 B. N. Color Index 698. $6 lbs. oi the dye known as Acid alizarine garnet R. A. Color Index 168.

lbs. sodium sulphate. 25. lbs. 36% acetic acid.

- The dye bath containing the material to be dyed was brought to the boil, 'boiled three- 70 quarters 01' an hour, 10 pounds formic acid added. boiled one-halt hour, 4% pounds sodium dichromate added half hour.

The dyeing was repeated on a fresh lot of materiaLtheonlychangebeingtheadditionto the hishly and the whole boiled a further:

dye bath of sodium phate.

dye bath atthe start, of 2% quarts 30% solution of sodium hexametaphosphate. This resulted in an improved product.

The dye, Diamond blue black R. B. N., dyes red but the subsequent treatment with dichromate turnsit to a blue, thus intensifying the black shade or the dye that is present in the largest portion.

Any failure of completeness of the chroming would allow the orisinal red color oi. the blue black to remain and give a reddish cast to portions of the dyed material. The material dyed without the use oi" sodium hexametaphosphate not only dyed unevenly, but chromed unevenly as well, whereas the slubbing dyed with the addition oi the metaphosphate not only dyed evenly, but chromed more thoroughlyand evenly and showed no traces of spots oi reddish'hue.

E. In order to determine the eifect of sodium phosphate on the deleterious action or small quantities oi contaminating metals such as may arise from walls or dyeing vesels, etc. on the colors of delicate shades. I made experimental shade-changing eiiects oi the lie impurities and, gating agents were employed, phate had a selective action on t 1". The'i'ollowing is an extraneous metalthe metaphos- I dyed pounds tured from oiled tops made up as follows:

worsted slubbing manufacin 1000 gallons of dye bath 1 lb. 01' the dye known as Diamond G. A. Color Index 110. 2 lbs. sodium dichromate. 40 lbs. sodium sulphate.

7 lbs. 26? ammonia. 10 lbs. 56% acetic acid.

This was brought to a boil, bofled one-halrhour. 2 lbs. acetic acid added and boiled one-halt 2 lbs. formic acidand with one-quarter them. I An extremely deleterious sludge was found precipitated on the goods. Ithen repeated this operation on fresh material, but with the addition or 2% quarts 30% sodium hexametaphos- The result was a complete absence of sludge on the goods of an otherwise n The preferred material is washing operation.

I I I I I I.. I I te '8 strongly heated, water is driven 0! and there is an atomic rearrangement within the molecul whereby sodium acid pyrophosphate is produced.

when other well-known mitiassoerecyanmea thenilbaotthesame,

hour boiling betw een' and enabled the omission,

the sodium hexa- Upon further heating until melting occurs, more water is driven 08, resulting in a further atomic rearrangement, whereby sodium hexametaphosphate is produced.

5 While I prefer to use .the'sodium hexametaphosphate, other alkali metal hexametaphosphosphates, appear to have a penetrating action 10 upon the textile fibers, or to assist the penetration of the-fibers by the dyestufls and mordants. They also appear to have a scouring or cleansing action upon the fibers, so that scouring may proceed coincidentally with the dyeing, thus elimi- 15 nating the expense of a separate scouring step in some instances. The scouring action resulting in removing undesirable substances, is shown Patentno'. 2,071,585.

ord'of the case in the Patent Office.

phates may be used, such as the potassium and ammonium salts. These'alkali-metal hexametaamines I 3 by' the elimination of the sludge in one of the examples above.

While I have specifically set forth certain examples showing the practice of my invention, it is to be understood that the invention is not lim- 5 ited thereto, but may be otherwise embodied or practiced within the scope of the following claims.

I claim:

1. In the process of dyeing textile materials, the step which consists in subjecting the textiles' 1o to a dyeing bath containing an alkali metal hexametaphosphate.

2. Inthe process of dyeing textile materials, the-step which consists in subjecting the textiles to a dyeing bath containing sodium hexameta- 15 phosphate.

EDWARD B. BELL.

CERTIFICATE OF CORRECTION.

February 23, 1937.

EDWARD B. BELL.

It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction as follows: first column, line 50, for fprecipiated" read precipitated; line 56, for the numeral ,"100" read 1000; and 'that the said Letters Patent should be read with these corrections therein that the same may conform to the rec- Page 2,

Signed and sealed this 30th day of March, A.D. 1957.

Henry V an llrsdale Acting Commissioner of Patents.

Upon further heating until melting occurs, more water is driven 08, resulting in a further atomic rearrangement, whereby sodium hexametaphosphate is produced.

5 While I prefer to use .the'sodium hexametaphosphate, other alkali metal hexametaphosphosphates, appear to have a penetrating action 10 upon the textile fibers, or to assist the penetration of the-fibers by the dyestufls and mordants. They also appear to have a scouring or cleansing action upon the fibers, so that scouring may proceed coincidentally with the dyeing, thus elimi- 15 nating the expense of a separate scouring step in some instances. The scouring action resulting in removing undesirable substances, is shown Patentno'. 2,071,585.

ord'of the case in the Patent Office.

phates may be used, such as the potassium and ammonium salts. These'alkali-metal hexametaamines I 3 by' the elimination of the sludge in one of the examples above.

While I have specifically set forth certain examples showing the practice of my invention, it is to be understood that the invention is not lim- 5 ited thereto, but may be otherwise embodied or practiced within the scope of the following claims.

I claim:

1. In the process of dyeing textile materials, the step which consists in subjecting the textiles' 1o to a dyeing bath containing an alkali metal hexametaphosphate.

2. Inthe process of dyeing textile materials, the-step which consists in subjecting the textiles to a dyeing bath containing sodium hexameta- 15 phosphate.

EDWARD B. BELL.

CERTIFICATE OF CORRECTION.

February 23, 1937.

EDWARD B. BELL.

It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction as follows: first column, line 50, for fprecipiated" read precipitated; line 56, for the numeral ,"100" read 1000; and 'that the said Letters Patent should be read with these corrections therein that the same may conform to the rec- Page 2,

Signed and sealed this 30th day of March, A.D. 1957.

Henry V an llrsdale Acting Commissioner of Patents. 

